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论文摘要

浆料配比对3D打印牙科二硅酸锂陶瓷的微观结构和性能的影响

Effect of slurry proportion on the microstructure and properties of dental lithium disilicate ceramics manufactured through 3D printing

作者:林保欣, 陈小瑄, 李如意, 万乾炳, 裴锡波

Author:Lin Baoxin, Chen Xiaoxuan, Li Ruyi, Wan Qianbing, Pei Xibo

收稿日期:2024-09-09          年卷(期)页码:2025,43(2):175-175-182

期刊名称:华西口腔医学杂志

Journal Name:West China Journal of Stomatology

关键字:3D打印,立体光固化成型技术,二硅酸锂,牙科陶瓷,浆料配比,

Key words:3D printing,stereo lithography apparatus,lithium disilicate,dental ceramics,slurry proportion,

基金项目:国家重点研发计划(2022YFC2410103);国家自然科学基金(82471021)

中文摘要

目的 使用基于立体光固化成型(SLA)原理的3D打印技术成型牙科用二硅酸锂陶瓷,以探讨不同浆料配比对热处理后样本的微观结构及性能的影响。 方法 以3D打印成型二硅酸锂为实验组,商品化的IPS e.max CAD切削类二硅酸锂陶瓷为对照组。实验组选用不同粒径的二硅酸锂陶瓷粉体材料(纳米级和微米级),与丙烯酸酯类光固化树脂混合,并调整浆料中实验原料的比例,配制5组陶瓷浆料(S1组-S5组)。根据浆料的流变特性、稳定性等状况评估其3D打印性能并筛选出适宜配比。对优选配比的实验组进行打印、脱脂及烧结程序,检测实验组的微观结构、晶体学信息以及收缩率,同时测量其弯曲强度、弹性模量、维氏硬度、断裂韧性等力学性能,与对照组进行比较。 结果 5组中筛选出2组用于3D打印的高固含量(75%)二硅酸锂陶瓷浆料(S2组和S3组)。X射线衍射及扫描电子显微镜结果显示,在S2组和S3组中,二硅酸锂均为主要晶相,显微结构为细长均匀、排列致密的晶体;二硅酸锂晶粒尺寸分别为(559.79±84.58)nm和(388.26±61.49)nm(P<0.05)。能谱分析结果显示,2组陶瓷样本均含有较高比例的Si和O元素。热处理后2组陶瓷样本的收缩率为18.00%~20.71%。2组的所有力学性能测试结果差异均无统计学意义(P>0.05),弯曲强度分别为(231.79±21.71)MPa和(214.86±46.64)MPa,低于IPS e.max CAD组(P<0.05);弹性模量分别为(87.40±12.99)GPa和(92.87±19.76)GPa,与IPS e.max CAD组差异无统计学意义(P>0.05);维氏硬度分别为(6.53±0.19)GPa和(6.25±0.12)GPa,高于IPS e.max CAD组(P<0.05);断裂韧性分别为(1.57±0.28)MPa·m0.5和(1.38±0.17)MPa·m0.5,与IPS e.max CAD组差异无统计学意义(P>0.05)。 结论 不同粒径级的二硅酸锂陶瓷粉体组合,可获得高固含量(75%)、有适宜的黏度和稳定性的浆料。3D打印技术可成功制备牙科二硅酸锂陶瓷样本,热处理后样本的收缩率较小,微观结构符合二硅酸锂陶瓷的晶相,力学性能接近切削类二硅酸锂陶瓷。

英文摘要

ObjectiveThis study aims to use 3D prin-ting technology based on the principle of stereo lithography apparatus (SLA) to shape dental lithium disilicate ceramics and study the effects of different slurry proportions on the microstructure and properties of heat-treated samples.MethodsThe experimental group comprised lithium disilicate ceramics manufactured through SLA 3D printing, and the control group comprised lithium disilicate ceramics (IPS e.max CAD) fabricated through commercial milling. An array of different particle sizes of lithium disilicate ceramic powder materials (nano and micron) was selected for mixing with photocurable acrylate resin. The proportion of experimental raw materials was adjusted to prepare five groups of ceramic slurries for 3D printing (Groups S1-S5) on the basis of rheological properties, stability, and other factors. Printing, debonding, and sintering were conducted on the experimental group with the optimal ratio, followed by measurements of microstructure, crystallographic information, shrinkage, and mechanical properties.ResultsFive groups of lithium disilicate ceramic slurries were prepared, of which two groups with high solid content (75%) (Groups S2 and S3) were selected for 3D printing. X-ray diffraction and scanning electron microscopy results showed that lithium disilicate was the main crystalline phase in Groups S2 and S3, and its microstructure was slender, uniform, and compact. The average grain sizes of Groups S2 and S3 were (559.79±84.58) nm and (388.26±61.49) nm, respectively (P<0 .05). energy spectroscopy revealed that the samples in the two groups contained a high proportion of si and o elements. after heat treatment, the shrinkage rate of the two groups of ceramic samples was 18.00%-20.71%. test results revealed no statistical difference in all mechanical properties between groups s2 and s3 (P>0.05). The flexural strengths of Groups S2 and S3 were (231.79±21.71) MPa and (214.86±46.64) MPa, respectively, which were lower than that of the IPS e.max CAD group (P<0 .05). the elasticity modulus of groups s2 and s3 were (87.40±12.99) gpa and (92.87±19.76) gpa, respectively, which did not significantly differ from that of the ips e.max cad group (P>0.05). The Vickers hardness values of Groups S2 and S3 were (6.53±0.19) GPa and (6.25±0.12) GPa, respectively, which were higher than that of the IPS e.max CAD group (P<0 .05). the fracture toughness values of groups s2 and s3 were (1.57±0.28) mpa·m0.5and (1.38±0.17) MPa·m0.5, respectively, which did not significantly differ from that of the IPS e.max CAD group (P>0.05).ConclusionThe combination of lithium disilicate ceramic powders with different particle sizes can yield a slurry with high solid content (75%) and suitable viscosity and stability. The dental lithium disilicate ceramic material is successfully prepared by using 3D printing technology. The 3D-printed samples show a small shrinkage rate after heat treatment. Their microstructure conforms to the crystal phase of lithium disilicate ceramics, and their mechanical properties are close to those of milled lithium disilicate ceramics.

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